# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_sm
_database_code_depnum_ccdc_archive 'CCDC 1060133'
_audit_update_record             
;
2015-10-08 deposited with the CCDC.
2015-10-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
"(C2 H8 N)+, [Sm3 (H2 O) (C3 H7 N O)2 (C21 H9 N O8)2] (C H O2)2]-, 18H(H2 O), 2 (C3 H7 N O)'"

_chemical_formula_sum            'C58 H94 N7 O43 Sm3'
_chemical_formula_weight         2028.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           204
_space_group_name_H-M_alt        'I m -3'
_space_group_name_Hall           '-I 2 2 3'

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z+1/2, x+1/2, y+1/2'
'z+1/2, x+1/2, -y+1/2'
'z+1/2, -x+1/2, y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z+1/2, x+1/2'
'-y+1/2, z+1/2, x+1/2'
'y+1/2, z+1/2, -x+1/2'

_cell_length_a                   38.3513(17)
_cell_length_b                   38.3513
_cell_length_c                   38.3513
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     56408(8)
_cell_formula_units_Z            24
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9856
_cell_measurement_theta_min      2.2551
_cell_measurement_theta_max      26.5216

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_F_000             24504
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    1.934
_shelx_estimated_absorpt_T_min   0.747
_shelx_estimated_absorpt_T_max   0.801
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            175427
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         1.679
_diffrn_reflns_theta_max         27.492
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11288
_reflns_number_gt                9271
_reflns_threshold_expression     'I > 2σ(I)'

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0751P)²+657.8595P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.000032(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         11288
_refine_ls_number_parameters     327
_refine_ls_number_restraints     282
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0577
_refine_ls_wR_factor_ref         0.1699
_refine_ls_wR_factor_gt          0.1479
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.111
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.30942(2) 0.0000 0.18572(2) 0.04281(16) Uani 1 2 d S T P . .
Sm2 Sm 0.25693(2) 0.08890(2) 0.24333(2) 0.03802(12) Uani 1 1 d . . . . .
O1 O 0.3424(2) 0.03846(18) 0.2193(2) 0.092(3) Uani 1 1 d D U . . .
O2 O 0.31849(18) 0.08729(17) 0.2378(2) 0.0570(18) Uani 1 1 d D U . . .
O3 O 0.38257(13) 0.19982(17) 0.23898(18) 0.0519(16) Uani 1 1 d D U . . .
O4 O 0.43899(15) 0.1999(2) 0.2328(2) 0.075(2) Uani 1 1 d D U . . .
O5 O 0.2005(2) 0.06107(15) 0.2512(2) 0.072(2) Uani 1 1 d D U . . .
O6 O 0.20025(18) 0.11683(15) 0.2435(2) 0.0598(19) Uani 1 1 d D U . . .
O7 O 0.08739(18) 0.18207(19) 0.25522(19) 0.0538(17) Uani 1 1 d D U . . .
O8 O 0.0537(3) 0.1606(2) 0.2962(3) 0.115(4) Uani 1 1 d D U . . .
O9 O 0.27066(19) 0.14789(15) 0.2245(2) 0.0565(16) Uani 1 1 d . U . . .
O10 O 0.26763(17) 0.02831(9) 0.23015(18) 0.0466(13) Uani 1 1 d D U . . .
O11 O 0.3237(5) 0.0000 0.1191(5) 0.155(7) Uani 1 2 d DS TU P . .
O12 O 0.3686(5) 0.0000 0.1533(5) 0.145(7) Uani 1 2 d DS TU P . .
O1W O 0.2494(5) 0.0000 0.1589(4) 0.122(6) Uani 1 2 d S TU P . .
H1 H 0.2385 -0.0178 0.1654 0.183 Uiso 1 1 calc DR U . . .
N1 N 0.5000 0.0973(5) 0.1971(4) 0.068(5) Uiso 0.5 2 d DS . P A 1
N1' N 0.5000 0.0850(5) 0.2093(5) 0.068(5) Uiso 0.5 2 d DS . P A 2
N2 N 0.0943(3) 0.0000 0.2894(4) 0.096(5) Uani 1 2 d DS TU P . .
N3 N 0.3018(2) 0.1831(2) 0.1873(2) 0.062(2) Uani 1 1 d . U . . .
C1 C 0.34390(18) 0.07071(19) 0.22634(14) 0.074(3) Uani 1 1 d D U . . .
C2 C 0.3764(3) 0.0919(4) 0.2201(2) 0.090(4) Uiso 0.5 1 d DG . P A 1
C3 C 0.3764(3) 0.1267(4) 0.23000(13) 0.057(2) Uiso 0.5 1 d G . P A 1
H3 H 0.3566 0.1365 0.2401 0.069 Uiso 0.5 1 calc R U P A 1
C4 C 0.4059(5) 0.1471(2) 0.2247(2) 0.061(3) Uiso 0.5 1 d DG . P A 1
C5 C 0.4354(3) 0.1325(4) 0.2096(3) 0.083(4) Uiso 0.5 1 d G . P A 1
H5 H 0.4552 0.1461 0.2060 0.099 Uiso 0.5 1 calc R U P A 1
C6 C 0.4354(3) 0.0977(5) 0.1997(2) 0.086(5) Uiso 0.5 1 d DG . P A 1
C7 C 0.4059(4) 0.0773(2) 0.2050(2) 0.126(7) Uiso 0.5 1 d G . P A 1
H7 H 0.4059 0.0540 0.1984 0.151 Uiso 0.5 1 calc R U P A 1
C2' C 0.3770(3) 0.0923(4) 0.22294(15) 0.090(4) Uiso 0.5 1 d DG . P A 2
C3' C 0.3792(3) 0.1279(4) 0.22915(12) 0.057(2) Uiso 0.5 1 d G . P A 2
H3' H 0.3594 0.1403 0.2359 0.069 Uiso 0.5 1 calc R U P A 2
C4' C 0.4108(5) 0.1451(2) 0.22525(17) 0.061(3) Uiso 0.5 1 d DG . P A 2
C5' C 0.4403(3) 0.1266(4) 0.2151(2) 0.083(4) Uiso 0.5 1 d G . P A 2
H5' H 0.4615 0.1381 0.2125 0.099 Uiso 0.5 1 calc R U P A 2
C6' C 0.4382(3) 0.0910(4) 0.2089(2) 0.086(5) Uiso 0.5 1 d DG . P A 2
C7' C 0.4065(5) 0.0738(2) 0.21283(19) 0.126(7) Uiso 0.5 1 d G . P A 2
H7' H 0.4050 0.0500 0.2087 0.151 Uiso 0.5 1 calc R U P A 2
C8 C 0.41070(18) 0.18419(17) 0.23271(12) 0.049(2) Uani 1 1 d D U . . .
C9 C 0.46860(11) 0.0857(4) 0.1836(3) 0.078(5) Uiso 0.5 1 d D . P A 1
C10 C 0.46857(11) 0.0620(5) 0.1559(4) 0.108(7) Uiso 0.5 1 d D . P A 1
H10 H 0.4475 0.0541 0.1468 0.129 Uiso 0.5 1 calc R U P A 1
C11 C 0.5000 0.0501(7) 0.1421(6) 0.097(9) Uiso 0.5 2 d DS . P A 1
H11 H 0.5000 0.0344 0.1236 0.117 Uiso 0.5 2 calc R U P A 1
C9' C 0.46861(11) 0.0707(5) 0.1982(4) 0.078(5) Uiso 0.5 1 d D . P A 2
C10' C 0.46857(11) 0.0420(5) 0.1761(5) 0.108(7) Uiso 0.5 1 d D . P A 2
H10' H 0.4475 0.0324 0.1687 0.129 Uiso 0.5 1 calc R U P A 2
C11' C 0.5000 0.0276(6) 0.1649(7) 0.097(9) Uiso 0.5 2 d DS . P A 2
H11' H 0.5000 0.0084 0.1501 0.117 Uiso 0.5 2 calc R U P A 2
C12 C 0.18474(19) 0.08946(18) 0.25104(13) 0.052(2) Uani 1 1 d D U . . .
C13 C 0.14685(15) 0.09121(16) 0.2600(2) 0.064(3) Uani 1 1 d DG U . . .
C14 C 0.12791(18) 0.12210(13) 0.2594(2) 0.060(3) Uani 1 1 d G U . . .
H14 H 0.1376 0.1421 0.2497 0.073 Uiso 1 1 calc R U . . .
C15 C 0.09442(18) 0.12313(15) 0.2732(2) 0.081(4) Uani 1 1 d DG U . . .
C16 C 0.07987(17) 0.09326(19) 0.2877(3) 0.101(5) Uani 1 1 d G U . . .
H16 H 0.0575 0.0939 0.2969 0.122 Uiso 1 1 calc R U . . .
C17 C 0.0988(2) 0.06237(16) 0.2883(3) 0.094(4) Uani 1 1 d DG U . . .
C18 C 0.13230(19) 0.06134(14) 0.2745(3) 0.084(4) Uani 1 1 d G U . . .
H18 H 0.1450 0.0407 0.2750 0.101 Uiso 1 1 calc R U . . .
C19 C 0.07747(19) 0.1581(2) 0.2746(2) 0.093(4) Uani 1 1 d D U . . .
C20 C 0.0817(3) 0.03123(10) 0.3029(3) 0.108(5) Uani 1 1 d D U . . .
C21 C 0.0569(4) 0.03153(11) 0.3294(4) 0.134(7) Uani 1 1 d D U . . .
H21 H 0.0487 0.0526 0.3382 0.160 Uiso 1 1 calc R U . . .
C22 C 0.0445(5) 0.0000 0.3426(5) 0.202(17) Uani 1 2 d DS TU P . .
H22 H 0.0280 0.0000 0.3603 0.242 Uiso 1 2 calc R U P . .
C23 C 0.2941(3) 0.1544(2) 0.2018(3) 0.062(3) Uani 1 1 d . U . . .
H23 H 0.3075 0.1354 0.1950 0.074 Uiso 1 1 calc R U . . .
C24 C 0.2792(5) 0.2150(3) 0.1964(3) 0.096(4) Uani 1 1 d . U . . .
H24A H 0.2557 0.2076 0.2008 0.144 Uiso 1 1 calc R U . . .
H24B H 0.2794 0.2311 0.1772 0.144 Uiso 1 1 calc R U . . .
H24C H 0.2884 0.2262 0.2168 0.144 Uiso 1 1 calc R U . . .
C25 C 0.3271(3) 0.1876(4) 0.1635(4) 0.096(5) Uani 1 1 d . U . . .
H25A H 0.3417 0.1672 0.1628 0.144 Uiso 1 1 calc R U . . .
H25B H 0.3409 0.2075 0.1696 0.144 Uiso 1 1 calc R U . . .
H25C H 0.3168 0.1911 0.1409 0.144 Uiso 1 1 calc R U . . .
C26 C 0.2569(4) 0.0000 0.2419(4) 0.046(3) Uani 1 2 d DS TU P . .
H26 H 0.2405 0.0000 0.2597 0.055 Uiso 1 2 calc R U P . .
C27 C 0.3557(6) 0.0000 0.1233(5) 0.119(8) Uani 1 2 d DS TU P . .
H27 H 0.3704 0.0000 0.1040 0.142 Uiso 1 2 calc R U P . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O1 2.330(8) . ?
Sm1 O1 2.330(8) 27 ?
Sm1 O8 2.331(8) 32 ?
Sm1 O8 2.331(8) 5 ?
Sm1 O1W 2.520(18) . ?
Sm1 O10 2.579(6) . ?
Sm1 O10 2.579(6) 27 ?
Sm1 O12 2.59(2) . ?
Sm1 O11 2.61(2) . ?
Sm2 O7 2.351(7) 5 ?
Sm2 O2 2.371(7) . ?
Sm2 O10 2.413(4) . ?
Sm2 O6 2.423(7) . ?
Sm2 O9 2.433(6) . ?
Sm2 O5 2.433(7) . ?
Sm2 O3 2.444(7) 41 ?
Sm2 O4 2.459(8) 41 ?
O1 C1 1.268(7) . ?
O2 C1 1.243(7) . ?
O3 C8 1.257(7) . ?
O3 Sm2 2.444(7) 45 ?
O4 C8 1.240(7) . ?
O4 Sm2 2.459(8) 45 ?
O5 C12 1.244(7) . ?
O6 C12 1.241(7) . ?
O7 C19 1.243(8) . ?
O7 Sm2 2.351(7) 9 ?
O8 C19 1.234(8) . ?
O8 Sm1 2.331(8) 9 ?
O9 C23 1.275(12) . ?
O10 C26 1.245(6) . ?
O11 C27 1.239(10) . ?
O12 C27 1.250(10) . ?
O1W H1 0.8401 . ?
N1 C9 1.385(6) . ?
N1 C9 1.385(6) 28_655 ?
N1' C9' 1.390(6) . ?
N1' C9' 1.390(6) 28_655 ?
N2 C20 1.391(6) . ?
N2 C20 1.391(6) 27 ?
N3 C23 1.267(12) . ?
N3 C25 1.344(14) . ?
N3 C24 1.541(16) . ?
C1 C2 1.505(8) . ?
C1 C2' 1.520(8) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C3 H3 0.9300 . ?
C4 C5 1.3900 . ?
C4 C8 1.468(8) . ?
C5 C6 1.3900 . ?
C5 H5 0.9300 . ?
C6 C7 1.3900 . ?
C6 C9 1.487(8) . ?
C7 H7 0.9300 . ?
C2' C3' 1.3900 . ?
C2' C7' 1.3900 . ?
C3' C4' 1.3900 . ?
C3' H3' 0.9300 . ?
C4' C5' 1.3900 . ?
C4' C8 1.526(8) . ?
C5' C6' 1.3900 . ?
C5' H5' 0.9300 . ?
C6' C7' 1.3900 . ?
C6' C9' 1.463(14) . ?
C7' H7' 0.9300 . ?
C8 Sm2 2.808(6) 45 ?
C9 C10 1.396(7) . ?
C10 C11 1.393(6) . ?
C10 H10 0.9300 . ?
C11 C10 1.393(6) 28_655 ?
C11 H11 0.9300 . ?
C9' C10' 1.389(7) . ?
C10' C11' 1.394(6) . ?
C10' H10' 0.9300 . ?
C11' C10' 1.394(6) 28_655 ?
C11' H11' 0.9300 . ?
C12 C13 1.495(7) . ?
C13 C14 1.3900 . ?
C13 C18 1.3900 . ?
C14 C15 1.3900 . ?
C14 H14 0.9300 . ?
C15 C16 1.3900 . ?
C15 C19 1.491(8) . ?
C16 C17 1.3900 . ?
C16 H16 0.9300 . ?
C17 C18 1.3900 . ?
C17 C20 1.473(7) . ?
C18 H18 0.9300 . ?
C20 C21 1.391(7) . ?
C21 C22 1.394(6) . ?
C21 H21 0.9300 . ?
C22 C21 1.394(6) 27 ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 O10 1.245(6) 27 ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Sm1 O1 78.5(4) . 27 ?
O1 Sm1 O8 155.0(4) . 32 ?
O1 Sm1 O8 77.7(4) 27 32 ?
O1 Sm1 O8 77.7(4) . 5 ?
O1 Sm1 O8 155.0(4) 27 5 ?
O8 Sm1 O8 124.2(6) 32 5 ?
O1 Sm1 O1W 136.1(3) . . ?
O1 Sm1 O1W 136.1(3) 27 . ?
O8 Sm1 O1W 68.5(3) 32 . ?
O8 Sm1 O1W 68.5(3) 5 . ?
O1 Sm1 O10 72.9(3) . . ?
O1 Sm1 O10 103.8(3) 27 . ?
O8 Sm1 O10 120.7(3) 32 . ?
O8 Sm1 O10 76.5(2) 5 . ?
O1W Sm1 O10 72.7(4) . . ?
O1 Sm1 O10 103.8(3) . 27 ?
O1 Sm1 O10 72.9(3) 27 27 ?
O8 Sm1 O10 76.5(2) 32 27 ?
O8 Sm1 O10 120.7(3) 5 27 ?
O1W Sm1 O10 72.7(4) . 27 ?
O10 Sm1 O10 49.80(17) . 27 ?
O1 Sm1 O12 77.9(4) . . ?
O1 Sm1 O12 77.9(4) 27 . ?
O8 Sm1 O12 89.5(3) 32 . ?
O8 Sm1 O12 89.5(3) 5 . ?
O1W Sm1 O12 127.2(6) . . ?
O10 Sm1 O12 149.6(3) . . ?
O10 Sm1 O12 149.6(3) 27 . ?
O1 Sm1 O11 115.2(4) . . ?
O1 Sm1 O11 115.2(4) 27 . ?
O8 Sm1 O11 68.9(3) 32 . ?
O8 Sm1 O11 68.9(3) 5 . ?
O1W Sm1 O11 78.0(6) . . ?
O10 Sm1 O11 140.9(4) . . ?
O10 Sm1 O11 140.9(4) 27 . ?
O12 Sm1 O11 49.1(3) . . ?
O7 Sm2 O2 86.4(2) 5 . ?
O7 Sm2 O10 76.8(2) 5 . ?
O2 Sm2 O10 77.7(2) . . ?
O7 Sm2 O6 89.3(3) 5 . ?
O2 Sm2 O6 154.8(2) . . ?
O10 Sm2 O6 125.4(2) . . ?
O7 Sm2 O9 74.5(2) 5 . ?
O2 Sm2 O9 77.4(2) . . ?
O10 Sm2 O9 142.8(2) . . ?
O6 Sm2 O9 77.5(2) . . ?
O7 Sm2 O5 95.0(3) 5 . ?
O2 Sm2 O5 152.4(2) . . ?
O10 Sm2 O5 75.8(2) . . ?
O6 Sm2 O5 52.78(17) . . ?
O9 Sm2 O5 129.6(2) . . ?
O7 Sm2 O3 154.7(2) 5 41 ?
O2 Sm2 O3 91.6(3) . 41 ?
O10 Sm2 O3 127.4(2) . 41 ?
O6 Sm2 O3 81.8(2) . 41 ?
O9 Sm2 O3 80.5(2) . 41 ?
O5 Sm2 O3 98.2(3) . 41 ?
O7 Sm2 O4 151.5(2) 5 41 ?
O2 Sm2 O4 84.8(3) . 41 ?
O10 Sm2 O4 74.9(2) . 41 ?
O6 Sm2 O4 109.5(3) . 41 ?
O9 Sm2 O4 129.3(2) . 41 ?
O5 Sm2 O4 80.9(3) . 41 ?
O3 Sm2 O4 52.71(17) 41 41 ?
C1 O1 Sm1 139.5(6) . . ?
C1 O2 Sm2 145.6(5) . . ?
C8 O3 Sm2 93.1(4) . 45 ?
C8 O4 Sm2 92.8(5) . 45 ?
C12 O5 Sm2 92.7(5) . . ?
C12 O6 Sm2 93.2(5) . . ?
C19 O7 Sm2 136.9(6) . 9 ?
C19 O8 Sm1 146.1(7) . 9 ?
C23 O9 Sm2 122.5(6) . . ?
C26 O10 Sm2 135.1(5) . . ?
C26 O10 Sm1 94.4(5) . . ?
Sm2 O10 Sm1 130.5(2) . . ?
C27 O11 Sm1 94.6(11) . . ?
C27 O12 Sm1 95.6(11) . . ?
Sm1 O1W H1 109.5 . . ?
C9 N1 C9 120.8(7) . 28_655 ?
C9' N1' C9' 120.0(7) . 28_655 ?
C20 N2 C20 118.9(6) . 27 ?
C23 N3 C25 125.5(11) . . ?
C23 N3 C24 117.2(10) . . ?
C25 N3 C24 117.3(10) . . ?
O2 C1 O1 122.6(7) . . ?
O2 C1 C2 115.4(9) . . ?
O1 C1 C2 122.0(10) . . ?
O2 C1 C2' 113.9(9) . . ?
O1 C1 C2' 123.4(10) . . ?
C3 C2 C7 120.0 . . ?
C3 C2 C1 118.4(13) . . ?
C7 C2 C1 121.6(13) . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 C8 112.0(14) . . ?
C3 C4 C8 128.0(14) . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 120.0 . . ?
C5 C6 C9 114.3(15) . . ?
C7 C6 C9 125.7(15) . . ?
C6 C7 C2 120.0 . . ?
C6 C7 H7 120.0 . . ?
C2 C7 H7 120.0 . . ?
C3' C2' C7' 120.0 . . ?
C3' C2' C1 124.8(13) . . ?
C7' C2' C1 115.2(13) . . ?
C2' C3' C4' 120.0 . . ?
C2' C3' H3' 120.0 . . ?
C4' C3' H3' 120.0 . . ?
C3' C4' C5' 120.0 . . ?
C3' C4' C8 116.3(14) . . ?
C5' C4' C8 123.7(14) . . ?
C6' C5' C4' 120.0 . . ?
C6' C5' H5' 120.0 . . ?
C4' C5' H5' 120.0 . . ?
C5' C6' C7' 120.0 . . ?
C5' C6' C9' 121.6(15) . . ?
C7' C6' C9' 118.4(15) . . ?
C6' C7' C2' 120.0 . . ?
C6' C7' H7' 120.0 . . ?
C2' C7' H7' 120.0 . . ?
O4 C8 O3 121.3(7) . . ?
O4 C8 C4 125.5(9) . . ?
O3 C8 C4 113.2(9) . . ?
O4 C8 C4' 118.3(9) . . ?
O3 C8 C4' 120.5(9) . . ?
O4 C8 Sm2 61.0(4) . 45 ?
O3 C8 Sm2 60.4(4) . 45 ?
C4 C8 Sm2 172.0(6) . 45 ?
C4' C8 Sm2 177.3(4) . 45 ?
N1 C9 C10 119.7(5) . . ?
N1 C9 C6 119.2(8) . . ?
C10 C9 C6 121.1(8) . . ?
C11 C10 C9 120.1(5) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C11 C10 119.8(7) 28_655 . ?
C10 C11 H11 120.1 28_655 . ?
C10 C11 H11 120.1 . . ?
C10' C9' N1' 120.1(5) . . ?
C10' C9' C6' 126.3(8) . . ?
N1' C9' C6' 113.2(9) . . ?
C9' C10' C11' 120.1(5) . . ?
C9' C10' H10' 120.0 . . ?
C11' C10' H10' 120.0 . . ?
C10' C11' C10' 119.8(7) 28_655 . ?
C10' C11' H11' 120.1 28_655 . ?
C10' C11' H11' 120.1 . . ?
O6 C12 O5 120.6(7) . . ?
O6 C12 C13 118.8(7) . . ?
O5 C12 C13 120.6(7) . . ?
C14 C13 C18 120.0 . . ?
C14 C13 C12 122.8(5) . . ?
C18 C13 C12 116.5(5) . . ?
C13 C14 C15 120.0 . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C16 C15 C14 120.0 . . ?
C16 C15 C19 123.5(5) . . ?
C14 C15 C19 116.3(5) . . ?
C15 C16 C17 120.0 . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C18 C17 C16 120.0 . . ?
C18 C17 C20 122.2(6) . . ?
C16 C17 C20 117.7(6) . . ?
C17 C18 C13 120.0 . . ?
C17 C18 H18 120.0 . . ?
C13 C18 H18 120.0 . . ?
O8 C19 O7 124.8(8) . . ?
O8 C19 C15 114.5(8) . . ?
O7 C19 C15 120.7(8) . . ?
N2 C20 C21 121.0(4) . . ?
N2 C20 C17 113.8(6) . . ?
C21 C20 C17 125.1(6) . . ?
C20 C21 C22 119.4(5) . . ?
C20 C21 H21 120.3 . . ?
C22 C21 H21 120.3 . . ?
C21 C22 C21 120.3(7) 27 . ?
C21 C22 H22 119.9 27 . ?
C21 C22 H22 119.9 . . ?
N3 C23 O9 129.5(10) . . ?
N3 C23 H23 115.3 . . ?
O9 C23 H23 115.3 . . ?
N3 C24 H24A 109.5 . . ?
N3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N3 C25 H25A 109.5 . . ?
N3 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
N3 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O10 C26 O10 121.4(9) 27 . ?
O10 C26 H26 119.3 27 . ?
O10 C26 H26 119.3 . . ?
O11 C27 O12 120.7(14) . . ?
O11 C27 H27 119.7 . . ?
O12 C27 H27 119.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Sm2 O2 C1 O1 -20.5(7) . . . . ?
Sm2 O2 C1 C2 157.2(7) . . . . ?
Sm2 O2 C1 C2' 161.5(7) . . . . ?
Sm1 O1 C1 O2 54.6(9) . . . . ?
Sm1 O1 C1 C2 -123.0(9) . . . . ?
Sm1 O1 C1 C2' -127.6(8) . . . . ?
O2 C1 C2 C3 5.0(4) . . . . ?
O1 C1 C2 C3 -177.3(4) . . . . ?
O2 C1 C2 C7 -175.1(4) . . . . ?
O1 C1 C2 C7 2.7(4) . . . . ?
C7 C2 C3 C4 0.0 . . . . ?
C1 C2 C3 C4 179.92(8) . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C2 C3 C4 C8 178.8(3) . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C8 C4 C5 C6 -179.0(2) . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C4 C5 C6 C9 179.5(3) . . . . ?
C5 C6 C7 C2 0.0 . . . . ?
C9 C6 C7 C2 -179.5(4) . . . . ?
C3 C2 C7 C6 0.0 . . . . ?
C1 C2 C7 C6 -179.92(8) . . . . ?
O2 C1 C2' C3' -4.8(4) . . . . ?
O1 C1 C2' C3' 177.3(4) . . . . ?
O2 C1 C2' C7' 175.2(4) . . . . ?
O1 C1 C2' C7' -2.7(4) . . . . ?
C7' C2' C3' C4' 0.0 . . . . ?
C1 C2' C3' C4' 179.98(9) . . . . ?
C2' C3' C4' C5' 0.0 . . . . ?
C2' C3' C4' C8 -179.9(2) . . . . ?
C3' C4' C5' C6' 0.0 . . . . ?
C8 C4' C5' C6' 179.9(3) . . . . ?
C4' C5' C6' C7' 0.0 . . . . ?
C4' C5' C6' C9' 180.0(4) . . . . ?
C5' C6' C7' C2' 0.0 . . . . ?
C9' C6' C7' C2' -180.0(3) . . . . ?
C3' C2' C7' C6' 0.0 . . . . ?
C1 C2' C7' C6' -179.98(8) . . . . ?
Sm2 O4 C8 O3 -3.9(3) 45 . . . ?
Sm2 O4 C8 C4 174.5(3) 45 . . . ?
Sm2 O4 C8 C4' 177.0(3) 45 . . . ?
Sm2 O3 C8 O4 3.9(3) 45 . . . ?
Sm2 O3 C8 C4 -174.6(3) 45 . . . ?
Sm2 O3 C8 C4' -177.0(3) 45 . . . ?
C5 C4 C8 O4 -13.6(4) . . . . ?
C3 C4 C8 O4 167.6(4) . . . . ?
C5 C4 C8 O3 164.9(4) . . . . ?
C3 C4 C8 O3 -13.9(4) . . . . ?
C3' C4' C8 O4 173.1(4) . . . . ?
C5' C4' C8 O4 -6.7(4) . . . . ?
C3' C4' C8 O3 -6.0(4) . . . . ?
C5' C4' C8 O3 174.2(4) . . . . ?
C9 N1 C9 C10 -0.1(2) 28_655 . . . ?
C9 N1 C9 C6 177.6(10) 28_655 . . . ?
C5 C6 C9 N1 39.7(6) . . . . ?
C7 C6 C9 N1 -140.8(6) . . . . ?
C5 C6 C9 C10 -142.7(12) . . . . ?
C7 C6 C9 C10 36.8(13) . . . . ?
N1 C9 C10 C11 0.0(3) . . . . ?
C6 C9 C10 C11 -177.7(10) . . . . ?
C9 C10 C11 C10 0.1(6) . . . 28_655 ?
C9' N1' C9' C10' 0.0(2) 28_655 . . . ?
C9' N1' C9' C6' -173.5(9) 28_655 . . . ?
C5' C6' C9' C10' -146.5(12) . . . . ?
C7' C6' C9' C10' 33.5(13) . . . . ?
C5' C6' C9' N1' 26.5(5) . . . . ?
C7' C6' C9' N1' -153.6(5) . . . . ?
N1' C9' C10' C11' 0.0(3) . . . . ?
C6' C9' C10' C11' 172.5(11) . . . . ?
C9' C10' C11' C10' 0.0(6) . . . 28_655 ?
Sm2 O6 C12 O5 -8.5(4) . . . . ?
Sm2 O6 C12 C13 171.4(4) . . . . ?
Sm2 O5 C12 O6 8.5(4) . . . . ?
Sm2 O5 C12 C13 -171.4(4) . . . . ?
O6 C12 C13 C14 1.9(7) . . . . ?
O5 C12 C13 C14 -178.2(6) . . . . ?
O6 C12 C13 C18 -168.3(5) . . . . ?
O5 C12 C13 C18 11.6(6) . . . . ?
C18 C13 C14 C15 0.0 . . . . ?
C12 C13 C14 C15 -169.9(7) . . . . ?
C13 C14 C15 C16 0.0 . . . . ?
C13 C14 C15 C19 174.0(7) . . . . ?
C14 C15 C16 C17 0.0 . . . . ?
C19 C15 C16 C17 -173.6(8) . . . . ?
C15 C16 C17 C18 0.0 . . . . ?
C15 C16 C17 C20 -178.0(10) . . . . ?
C16 C17 C18 C13 0.0 . . . . ?
C20 C17 C18 C13 177.9(10) . . . . ?
C14 C13 C18 C17 0.0 . . . . ?
C12 C13 C18 C17 170.5(7) . . . . ?
Sm1 O8 C19 O7 34.2(13) 9 . . . ?
Sm1 O8 C19 C15 -146.0(13) 9 . . . ?
Sm2 O7 C19 O8 28.3(7) 9 . . . ?
Sm2 O7 C19 C15 -151.5(7) 9 . . . ?
C16 C15 C19 O8 15.9(6) . . . . ?
C14 C15 C19 O8 -157.9(7) . . . . ?
C16 C15 C19 O7 -164.3(6) . . . . ?
C14 C15 C19 O7 21.9(7) . . . . ?
C20 N2 C20 C17 175.8(9) 27 . . . ?
C18 C17 C20 N2 -25.0(9) . . . . ?
C16 C17 C20 N2 152.9(6) . . . . ?
C18 C17 C20 C21 150.6(9) . . . . ?
C16 C17 C20 C21 -31.5(14) . . . . ?
N2 C20 C21 C22 0.0(3) . . . . ?
C17 C20 C21 C22 -175.4(10) . . . . ?
C20 C21 C22 C21 0.0(6) . . . 27 ?
C25 N3 C23 O9 -179.9(13) . . . . ?
C24 N3 C23 O9 -3.1(19) . . . . ?
Sm2 O9 C23 N3 172.9(10) . . . . ?
Sm2 O10 C26 O10 -178.7(6) . . . 27 ?
Sm1 O10 C26 O10 -0.7(17) . . . 27 ?
Sm1 O11 C27 O12 0.000(1) . . . . ?
Sm1 O12 C27 O11 0.000(1) . . . . ?

_refine_diff_density_max         1.737
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.142



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cu
_database_code_depnum_ccdc_archive 'CCDC 1060134'
_audit_update_record             
;
2015-10-08 deposited with the CCDC.
2015-10-09 downloaded from the CCDC.
;

_vrf_PLAT417_cu                  
;
PROBLEM: Short Inter D-H..H-D       H1     ..  H1      ..       1.58 Ang.  
RESPONSE: The two hydrogen atoms belong to the same water O atom, which lies on 
a special position.  The alert is an artifact.
;

_vrf_PLAT420_cu                  
;
PROBLEM: D-H without Acceptor       O1w    -   H1     ...     Please Check 
RESPONSE: It is probably bonded to the SQUEEZEd solvent molecules.
;

_vrf_PLAT430_cu                  
;
PROBLEM: Short Inter D...A Contact  O1     ..  O1      ..       2.72 Ang.  
RESPONSE: The structure features a water-Cu^...^Cu^...^water unit and four
carboxyl -CO~2~ groups chelate Cu^...^Cu species.  The contact is normal.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cu2 (H2 O)2 (C21 H17 N O8), 2.222(C4 H9 N O)'
_chemical_formula_sum            'C29.89 H41 Cu2 N3.22 O12.22'
_chemical_formula_weight         768.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_H-M_alt        'R -3 m :H'
_space_group_name_Hall           '-R 3 2"'

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'

_cell_length_a                   18.6342(14)
_cell_length_b                   18.6342
_cell_length_c                   37.709(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     11339.7(19)
_cell_formula_units_Z            9
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2809
_cell_measurement_theta_min      2.5806
_cell_measurement_theta_max      21.3361

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_transmission_factor_min   none
_exptl_transmission_factor_max   none
_exptl_crystal_density_diffrn    1.012
_exptl_crystal_F_000             3588
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    0.888
_shelx_estimated_absorpt_T_min   0.835
_shelx_estimated_absorpt_T_max   0.856
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23422
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_av_R_equivalents  0.0844
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.186
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             3154
_reflns_number_gt                2226
_reflns_threshold_expression     'I > 2σ(I)'

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0572P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00052(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3154
_refine_ls_number_parameters     102
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0485
_refine_ls_wR_factor_ref         0.1409
_refine_ls_wR_factor_gt          0.1336
_refine_ls_goodness_of_fit_ref   1.295
_refine_ls_restrained_S_all      1.311
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.85619(2) 0.71239(3) 0.13782(2) 0.03326(19) Uani 1 2 d S T P . .
O1 O 0.88984(14) 0.63392(12) 0.12274(5) 0.0520(6) Uani 1 1 d . . . . .
O2 O 0.85093(14) 0.55579(12) 0.17124(5) 0.0500(6) Uani 1 1 d . . . . .
O1w O 0.88957(13) 0.7791(3) 0.08942(9) 0.0830(12) Uani 1 2 d S T P . .
H1w H 0.8546 0.7935 0.0844 0.125 Uiso 0.5 1 calc R U P . .
C1 C 0.87865(18) 0.57293(17) 0.14039(8) 0.0425(7) Uani 1 1 d . . . . .
C2 C 0.89843(19) 0.51311(18) 0.12314(8) 0.0461(7) Uani 1 1 d . . . . .
C3 C 0.8841(3) 0.44205(14) 0.14077(11) 0.0450(10) Uani 1 2 d S T P . .
C4 C 0.9282(2) 0.52800(19) 0.08868(8) 0.0566(9) Uani 1 1 d . . . . .
H4 H 0.9385 0.5764 0.0772 0.068 Uiso 1 1 calc R U . . .
C5 C 0.9428(3) 0.47141(17) 0.07121(12) 0.0636(15) Uani 1 2 d DS T P A .
C6 C 0.9733(4) 0.48664(19) 0.03481(9) 0.0720(17) Uani 1 2 d DS T P . .
C7 C 0.9513(7) 0.5312(7) 0.0124(2) 0.079(2) Uani 0.25 1 d D U P A -1
H7 H 0.9220 0.5557 0.0211 0.095 Uiso 0.25 1 d R U P A -1
C8 C 0.9797(6) 0.5462(6) -0.02232(18) 0.089(3) Uani 0.25 1 d D . P A -1
H8 H 0.9663 0.5773 -0.0374 0.106 Uiso 0.25 1 d R U P A -1
C7' C 0.9506(14) 0.5305(14) 0.0123(3) 0.079(2) Uani 0.25 1 d D . P A -2
H7' H 0.9078 0.5400 0.0186 0.095 Uiso 0.25 1 d R U P A -2
N1 N 0.9797(6) 0.5461(6) -0.02231(18) 0.089(3) Uani 0.25 1 d D U P A -2


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.942(2) . ?
Cu1 O1 1.942(2) 23_655 ?
Cu1 O2 1.9482(19) 11_565 ?
Cu1 O2 1.9483(19) 25_665 ?
Cu1 O1w 2.119(3) . ?
Cu1 Cu1 2.6287(8) 25_665 ?
O1 C1 1.242(3) . ?
O2 C1 1.248(3) . ?
O2 Cu1 1.9482(19) 25_665 ?
O1w H1w 0.8401 . ?
C1 C2 1.487(4) . ?
C2 C3 1.383(3) . ?
C2 C4 1.385(4) . ?
C3 C2 1.383(3) 24 ?
C4 C5 1.381(4) . ?
C4 H4 0.9300 . ?
C5 C4 1.381(4) 24 ?
C5 C6 1.458(5) . ?
C6 N1 1.376(7) 19_765 ?
C6 C8 1.379(7) 19_765 ?
C6 C7' 1.383(8) . ?
C6 C7 1.383(7) . ?
C7 C8 1.386(7) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C7' N1 1.386(7) . ?
C7' H7' 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O1 88.74(14) . 23_655 ?
O1 Cu1 O2 90.06(10) . 11_565 ?
O1 Cu1 O2 167.96(8) 23_655 11_565 ?
O1 Cu1 O2 167.97(8) . 25_665 ?
O1 Cu1 O2 90.06(10) 23_655 25_665 ?
O2 Cu1 O2 88.62(13) 11_565 25_665 ?
O1 Cu1 O1w 94.54(11) . . ?
O1 Cu1 O1w 94.54(11) 23_655 . ?
O2 Cu1 O1w 97.49(11) 11_565 . ?
O2 Cu1 O1w 97.49(11) 25_665 . ?
O1 Cu1 Cu1 82.90(6) . 25_665 ?
O1 Cu1 Cu1 82.90(6) 23_655 25_665 ?
O2 Cu1 Cu1 85.07(6) 11_565 25_665 ?
O2 Cu1 Cu1 85.07(6) 25_665 25_665 ?
O1w Cu1 Cu1 176.40(13) . 25_665 ?
C1 O1 Cu1 124.24(19) . . ?
C1 O2 Cu1 121.21(19) . 25_665 ?
Cu1 O1w H1w 109.5 . . ?
O1 C1 O2 126.3(3) . . ?
O1 C1 C2 117.4(3) . . ?
O2 C1 C2 116.2(3) . . ?
C3 C2 C4 120.6(3) . . ?
C3 C2 C1 120.4(3) . . ?
C4 C2 C1 119.0(3) . . ?
C2 C3 C2 118.8(4) . 24 ?
C5 C4 C2 120.4(3) . . ?
C5 C4 H4 119.8 . . ?
C2 C4 H4 119.8 . . ?
C4 C5 C4 119.1(4) . 24 ?
C4 C5 C6 120.45(19) . . ?
C4 C5 C6 120.44(19) 24 . ?
N1 C6 C7' 120.0(4) 19_765 . ?
C8 C6 C7 120.1(3) 19_765 . ?
N1 C6 C5 120.6(3) 19_765 . ?
C8 C6 C5 120.5(3) 19_765 . ?
C7' C6 C5 119.3(4) . . ?
C7 C6 C5 119.3(4) . . ?
C6 C7 C8 120.1(4) . . ?
C6 C7 H7 120.1 . . ?
C8 C7 H7 119.6 . . ?
C7 C8 H8 120.5 . . ?
C6 C7' N1 119.9(4) . . ?
C6 C7' H7' 120.0 . . ?
N1 C7' H7' 118.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 O1 C1 O2 -6.2(5) . . . . ?
Cu1 O1 C1 C2 172.5(2) . . . . ?
Cu1 O2 C1 O1 5.7(4) 25_665 . . . ?
Cu1 O2 C1 C2 -173.06(19) 25_665 . . . ?
O1 C1 C2 C3 -177.3(3) . . . . ?
O2 C1 C2 C3 1.6(5) . . . . ?
O1 C1 C2 C4 0.2(4) . . . . ?
O2 C1 C2 C4 179.0(3) . . . . ?
C4 C2 C3 C2 -1.3(6) . . . 24 ?
C1 C2 C3 C2 176.1(2) . . . 24 ?
C3 C2 C4 C5 1.0(6) . . . . ?
C1 C2 C4 C5 -176.4(4) . . . . ?
C2 C4 C5 C4 -0.8(8) . . . 24 ?
C2 C4 C5 C6 179.3(4) . . . . ?
C4 C5 C6 N1 152.1(7) . . . 19_765 ?
C4 C5 C6 N1 -27.9(9) 24 . . 19_765 ?
C4 C5 C6 C8 152.1(7) . . . 19_765 ?
C4 C5 C6 C8 -27.9(9) 24 . . 19_765 ?
C4 C5 C6 C7' -31.6(13) . . . . ?
C4 C5 C6 C7' 148.5(14) 24 . . . ?
C4 C5 C6 C7 -30.9(12) . . . . ?
C4 C5 C6 C7 149.1(7) 24 . . . ?
C8 C6 C7 C8 -3.0(12) 19_765 . . . ?
C5 C6 C7 C8 -180.0(3) . . . . ?
N1 C6 C7' N1 -4(3) 19_765 . . . ?
C5 C6 C7' N1 179.4(18) . . . . ?

_refine_diff_density_max         0.716
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.088



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_zn_sq
_database_code_depnum_ccdc_archive 'CCDC 1061360'
_audit_update_record             
;
2015-10-08 deposited with the CCDC.
2015-10-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'[Zn2 (C4 H9 N O) (C21 H9 N O8)], 1.75(C4 H9 N O)'
_chemical_formula_sum            'C32 H33.75 N3.75 O10.75 Zn2'
_chemical_formula_weight         773.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_H-M_alt        'P 4/n'
_space_group_name_Hall           '-P 4a'

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'

_cell_length_a                   27.4541(15)
_cell_length_b                   27.4541
_cell_length_c                   9.7375(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7339.4(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9925
_cell_measurement_theta_min      2.2192
_cell_measurement_theta_max      26.4575

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_F_000             3184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.366
_shelx_estimated_absorpt_T_min   0.726
_shelx_estimated_absorpt_T_max   0.875
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            69414
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.219
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8429
_reflns_number_gt                6482
_reflns_threshold_expression     'I > 2σ(I)'

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0742P)²+11.1633P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8429
_refine_ls_number_parameters     337
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0586
_refine_ls_wR_factor_ref         0.1499
_refine_ls_wR_factor_gt          0.1397
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.43225(2) 0.03089(2) 0.94405(4) 0.02303(12) Uani 1 1 d . . . . .
Zn2 Zn 0.37540(2) 0.09299(2) 0.68999(4) 0.02840(12) Uani 1 1 d D . . . .
O1 O 0.42096(11) 0.10239(9) 0.9709(3) 0.0431(7) Uani 1 1 d . . . . .
O2 O 0.41239(11) 0.14464(10) 0.7763(3) 0.0438(7) Uani 1 1 d . . . . .
O3 O 0.42944(13) 0.32100(10) 0.7960(3) 0.0500(8) Uani 1 1 d . . . . .
O4 O 0.47712(11) 0.35525(9) 0.9551(3) 0.0429(7) Uani 1 1 d . . . . .
O5 O 0.56382(10) 0.01091(9) 1.2237(2) 0.0334(6) Uani 1 1 d . . . . .
O6 O 0.58741(12) -0.04095(10) 1.3870(3) 0.0456(7) Uani 1 1 d . . . . .
O7 O 0.56546(9) -0.00265(10) 1.8720(3) 0.0348(6) Uani 1 1 d . . . . .
O8 O 0.50612(9) 0.05031(10) 1.9206(2) 0.0329(6) Uani 1 1 d . . . . .
N1 N 0.50351(13) 0.17326(11) 1.3609(3) 0.0377(8) Uani 1 1 d . . . . .
C1 C 0.42470(14) 0.14060(14) 0.9015(4) 0.0339(8) Uani 1 1 d . . . . .
C2 C 0.44369(10) 0.18510(6) 0.9708(2) 0.0344(8) Uani 1 1 d G . . . .
C3 C 0.44253(10) 0.23001(8) 0.90493(18) 0.0342(8) Uani 1 1 d G . . . .
H3 H 0.4306 0.2324 0.8136 0.041 Uiso 1 1 calc R U . . .
C4 C 0.45886(10) 0.27147(6) 0.9727(2) 0.0348(9) Uani 1 1 d G . . . .
C5 C 0.47635(10) 0.26803(7) 1.1063(2) 0.0378(9) Uani 1 1 d G . . . .
H5 H 0.4875 0.2964 1.1526 0.045 Uiso 1 1 calc R U . . .
C6 C 0.47751(11) 0.22313(8) 1.17213(19) 0.0387(9) Uani 1 1 d G . . . .
C7 C 0.46118(11) 0.18166(6) 1.1044(2) 0.0397(9) Uani 1 1 d G . . . .
H7 H 0.4620 0.1510 1.1494 0.048 Uiso 1 1 calc R U . . .
C8 C 0.45547(15) 0.32035(13) 0.9030(4) 0.0346(9) Uani 1 1 d . . . . .
C9 C 0.49184(17) 0.21841(15) 1.3216(4) 0.0432(10) Uani 1 1 d . . . . .
C10 C 0.4908(2) 0.25720(17) 1.4115(5) 0.0654(16) Uani 1 1 d . . . . .
H10 H 0.4826 0.2890 1.3806 0.079 Uiso 1 1 calc R U . . .
C11 C 0.5022(3) 0.24859(18) 1.5487(5) 0.079(2) Uani 1 1 d . . . . .
H11 H 0.5016 0.2745 1.6134 0.095 Uiso 1 1 calc R U . . .
C12 C 0.5143(2) 0.20215(17) 1.5898(5) 0.0642(16) Uani 1 1 d . . . . .
H12 H 0.5222 0.1956 1.6830 0.077 Uiso 1 1 calc R U . . .
C13 C 0.51489(17) 0.16500(14) 1.4931(4) 0.0395(10) Uani 1 1 d . . . . .
C14 C 0.52674(10) 0.11298(6) 1.5284(2) 0.0326(8) Uani 1 1 d G . . . .
C15 C 0.52589(9) 0.09711(7) 1.66392(18) 0.0324(8) Uani 1 1 d G . . . .
H15 H 0.5155 0.1185 1.7347 0.039 Uiso 1 1 calc R U . . .
C16 C 0.54022(9) 0.04989(8) 1.69584(15) 0.0267(7) Uani 1 1 d G . . . .
C17 C 0.55539(9) 0.01854(6) 1.5922(2) 0.0273(7) Uani 1 1 d G . . . .
H17 H 0.5652 -0.0137 1.6140 0.033 Uiso 1 1 calc R U . . .
C18 C 0.55624(9) 0.03441(7) 1.45671(17) 0.0257(7) Uani 1 1 d G . . . .
C19 C 0.54192(10) 0.08164(8) 1.42479(15) 0.0317(8) Uani 1 1 d G . . . .
H19 H 0.5425 0.0925 1.3322 0.038 Uiso 1 1 calc R U . . .
C20 C 0.53641(13) 0.03121(13) 1.8412(3) 0.0258(7) Uani 1 1 d . . . . .
C21 C 0.57038(13) -0.00124(13) 1.3467(3) 0.0289(8) Uani 1 1 d . . . . .
O9 O 0.3358(4) 0.1197(5) 0.5390(9) 0.072(2) Uani 0.5 1 d D U P A 1
N2 N 0.3087(5) 0.1394(4) 0.3291(12) 0.120(2) Uani 0.5 1 d D U P A 1
C22 C 0.3447(4) 0.1249(3) 0.4141(10) 0.080(3) Uani 0.5 1 d D U P A 1
C23 C 0.3931(4) 0.1159(6) 0.3524(14) 0.143(5) Uani 0.5 1 d D U P A 1
H23A H 0.3916 0.1223 0.2534 0.215 Uiso 0.5 1 calc R U P A 1
H23B H 0.4172 0.1375 0.3948 0.215 Uiso 0.5 1 calc R U P A 1
H23C H 0.4025 0.0819 0.3679 0.215 Uiso 0.5 1 calc R U P A 1
C24 C 0.2597(4) 0.1487(7) 0.3841(15) 0.151(5) Uani 0.5 1 d D U P A 1
H24A H 0.2381 0.1589 0.3094 0.227 Uiso 0.5 1 calc R U P A 1
H24B H 0.2470 0.1189 0.4262 0.227 Uiso 0.5 1 calc R U P A 1
H24C H 0.2614 0.1746 0.4533 0.227 Uiso 0.5 1 calc R U P A 1
C25 C 0.3158(6) 0.1466(6) 0.1799(12) 0.149(6) Uani 0.5 1 d D U P A 1
H25A H 0.2851 0.1571 0.1381 0.223 Uiso 0.5 1 calc R U P A 1
H25B H 0.3408 0.1715 0.1648 0.223 Uiso 0.5 1 calc R U P A 1
H25C H 0.3263 0.1159 0.1381 0.223 Uiso 0.5 1 calc R U P A 1
O9' O 0.3502(4) 0.1221(5) 0.5213(9) 0.072(2) Uani 0.5 1 d D . P A 2
N2' N 0.3082(5) 0.1330(4) 0.3303(11) 0.120(2) Uani 0.5 1 d D . P A 2
C22' C 0.3115(4) 0.1321(3) 0.4678(10) 0.080(3) Uani 0.5 1 d D . P A 2
C23' C 0.2669(4) 0.1433(6) 0.5532(14) 0.143(5) Uani 0.5 1 d D . P A 2
H23D H 0.2393 0.1504 0.4924 0.215 Uiso 0.5 1 calc R U P A 2
H23E H 0.2590 0.1151 0.6109 0.215 Uiso 0.5 1 calc R U P A 2
H23F H 0.2734 0.1716 0.6117 0.215 Uiso 0.5 1 calc R U P A 2
C24' C 0.3500(5) 0.1222(7) 0.2435(12) 0.151(5) Uani 0.5 1 d D . P A 2
H24D H 0.3726 0.1494 0.2574 0.227 Uiso 0.5 1 d R U P A 2
H24E H 0.3392 0.1217 0.1475 0.227 Uiso 0.5 1 d R U P A 2
H24F H 0.3664 0.0915 0.2654 0.227 Uiso 0.5 1 d R U P A 2
C25' C 0.2619(5) 0.1451(6) 0.2624(14) 0.149(6) Uani 0.5 1 d D . P A 2
H25D H 0.2663 0.1440 0.1626 0.223 Uiso 0.5 1 calc R U P A 2
H25E H 0.2370 0.1214 0.2896 0.223 Uiso 0.5 1 calc R U P A 2
H25F H 0.2516 0.1778 0.2898 0.223 Uiso 0.5 1 calc R U P A 2


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O7 1.953(2) 5_658 ?
Zn1 O5 1.999(2) 5_657 ?
Zn1 O1 2.004(3) . ?
Zn1 O8 2.110(3) 1_554 ?
Zn1 O4 2.128(3) 4 ?
Zn2 O6 1.909(3) 5_657 ?
Zn2 O3 1.917(3) 4 ?
Zn2 O2 1.936(3) . ?
Zn2 O9' 1.953(6) . ?
Zn2 O9 1.969(6) . ?
O1 C1 1.252(5) . ?
O2 C1 1.270(5) . ?
O3 C8 1.263(5) . ?
O3 Zn2 1.917(3) 3 ?
O4 C8 1.237(5) . ?
O4 Zn1 2.128(3) 3 ?
O5 C21 1.256(4) . ?
O5 Zn1 1.999(2) 5_657 ?
O6 C21 1.250(4) . ?
O6 Zn2 1.909(3) 5_657 ?
O7 C20 1.261(4) . ?
O7 Zn1 1.953(2) 5_658 ?
O8 C20 1.251(4) . ?
O8 Zn1 2.110(3) 1_556 ?
N1 C9 1.336(5) . ?
N1 C13 1.344(5) . ?
C1 C2 1.490(4) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C4 C8 1.507(4) . ?
C5 C6 1.3900 . ?
C6 C7 1.3900 . ?
C6 C9 1.513(4) . ?
C9 C10 1.379(6) . ?
C10 C11 1.392(6) . ?
C11 C12 1.377(7) . ?
C12 C13 1.388(6) . ?
C13 C14 1.504(4) . ?
C14 C15 1.3900 . ?
C14 C19 1.3900 . ?
C15 C16 1.3900 . ?
C16 C17 1.3900 . ?
C16 C20 1.509(3) . ?
C17 C18 1.3900 . ?
C18 C19 1.3900 . ?
C18 C21 1.502(4) . ?
O9 C22 1.248(8) . ?
N2 C22 1.350(9) . ?
N2 C24 1.468(9) . ?
N2 C25 1.478(9) . ?
C22 C23 1.479(8) . ?
O9' C22' 1.215(8) . ?
N2' C22' 1.342(9) . ?
N2' C24' 1.456(9) . ?
N2' C25' 1.469(9) . ?
C22' C23' 1.513(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Zn1 O5 121.33(11) 5_658 5_657 ?
O7 Zn1 O1 105.91(12) 5_658 . ?
O5 Zn1 O1 132.61(11) 5_657 . ?
O7 Zn1 O8 99.71(10) 5_658 1_554 ?
O5 Zn1 O8 90.27(10) 5_657 1_554 ?
O1 Zn1 O8 85.14(11) . 1_554 ?
O7 Zn1 O4 86.81(11) 5_658 4 ?
O5 Zn1 O4 92.05(12) 5_657 4 ?
O1 Zn1 O4 86.62(12) . 4 ?
O8 Zn1 O4 170.64(11) 1_554 4 ?
O6 Zn2 O3 112.82(14) 5_657 4 ?
O6 Zn2 O2 115.98(14) 5_657 . ?
O3 Zn2 O2 114.20(14) 4 . ?
O6 Zn2 O9' 99.5(4) 5_657 . ?
O3 Zn2 O9' 108.0(3) 4 . ?
O2 Zn2 O9' 104.5(5) . . ?
O6 Zn2 O9 106.2(4) 5_657 . ?
O3 Zn2 O9 95.3(3) 4 . ?
O2 Zn2 O9 109.9(5) . . ?
C1 O1 Zn1 137.5(3) . . ?
C1 O2 Zn2 119.5(3) . . ?
C8 O3 Zn2 129.5(3) . 3 ?
C8 O4 Zn1 134.3(3) . 3 ?
C21 O5 Zn1 128.2(2) . 5_657 ?
C21 O6 Zn2 136.8(2) . 5_657 ?
C20 O7 Zn1 122.1(2) . 5_658 ?
C20 O8 Zn1 126.9(2) . 1_556 ?
C9 N1 C13 119.1(3) . . ?
O1 C1 O2 124.7(4) . . ?
O1 C1 C2 118.2(3) . . ?
O2 C1 C2 117.1(3) . . ?
C3 C2 C7 120.0 . . ?
C3 C2 C1 120.7(2) . . ?
C7 C2 C1 119.3(2) . . ?
C2 C3 C4 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 C8 120.2(2) . . ?
C3 C4 C8 119.7(2) . . ?
C4 C5 C6 120.0 . . ?
C7 C6 C5 120.0 . . ?
C7 C6 C9 118.1(2) . . ?
C5 C6 C9 121.7(2) . . ?
C6 C7 C2 120.0 . . ?
O4 C8 O3 126.9(3) . . ?
O4 C8 C4 118.4(3) . . ?
O3 C8 C4 114.8(3) . . ?
N1 C9 C10 122.6(4) . . ?
N1 C9 C6 114.7(3) . . ?
C10 C9 C6 122.7(3) . . ?
C9 C10 C11 118.3(4) . . ?
C12 C11 C10 119.3(4) . . ?
C11 C12 C13 119.1(4) . . ?
N1 C13 C12 121.5(4) . . ?
N1 C13 C14 115.4(3) . . ?
C12 C13 C14 123.0(3) . . ?
C15 C14 C19 120.0 . . ?
C15 C14 C13 120.72(19) . . ?
C19 C14 C13 119.1(2) . . ?
C14 C15 C16 120.0 . . ?
C17 C16 C15 120.0 . . ?
C17 C16 C20 119.42(18) . . ?
C15 C16 C20 120.47(18) . . ?
C16 C17 C18 120.0 . . ?
C17 C18 C19 120.0 . . ?
C17 C18 C21 118.50(19) . . ?
C19 C18 C21 121.43(19) . . ?
C18 C19 C14 120.0 . . ?
O8 C20 O7 125.7(3) . . ?
O8 C20 C16 118.9(3) . . ?
O7 C20 C16 115.4(3) . . ?
O6 C21 O5 125.8(3) . . ?
O6 C21 C18 116.2(3) . . ?
O5 C21 C18 118.0(3) . . ?
C22 O9 Zn2 131.5(7) . . ?
C22 N2 C24 119.8(10) . . ?
C22 N2 C25 123.0(11) . . ?
C24 N2 C25 117.2(8) . . ?
O9 C22 N2 119.3(10) . . ?
O9 C22 C23 123.5(8) . . ?
N2 C22 C23 117.3(10) . . ?
C22' O9' Zn2 139.7(7) . . ?
C22' N2' C24' 121.4(10) . . ?
C22' N2' C25' 120.8(11) . . ?
C24' N2' C25' 117.8(8) . . ?
O9' C22' N2' 119.5(10) . . ?
O9' C22' C23' 121.3(8) . . ?
N2' C22' C23' 119.3(10) . . ?

_refine_diff_density_max         0.889
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.096



